CN103965659A - Method for preparing high water dispersibility titanium dioxide - Google Patents
Method for preparing high water dispersibility titanium dioxide Download PDFInfo
- Publication number
- CN103965659A CN103965659A CN201410165452.5A CN201410165452A CN103965659A CN 103965659 A CN103965659 A CN 103965659A CN 201410165452 A CN201410165452 A CN 201410165452A CN 103965659 A CN103965659 A CN 103965659A
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- solution
- water
- dispersibility
- slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 331
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 157
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000002002 slurry Substances 0.000 claims abstract description 96
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 38
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 22
- 239000011734 sodium Substances 0.000 claims abstract description 22
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 22
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011574 phosphorus Substances 0.000 claims abstract description 21
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 21
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 28
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 28
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 23
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 14
- 238000004537 pulping Methods 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 10
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 10
- 239000001488 sodium phosphate Substances 0.000 claims description 6
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 6
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 6
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 5
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 5
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 4
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 4
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 4
- ZXVOCOLRQJZVBW-UHFFFAOYSA-N azane;ethanol Chemical compound N.CCO ZXVOCOLRQJZVBW-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 abstract description 23
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 abstract description 12
- 238000000576 coating method Methods 0.000 abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 125
- 239000000047 product Substances 0.000 description 14
- 238000005303 weighing Methods 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- HMNOVBZVCHMSQG-UHFFFAOYSA-N [Na].NCCO Chemical compound [Na].NCCO HMNOVBZVCHMSQG-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000001164 aluminium sulphate Substances 0.000 description 1
- 235000011128 aluminium sulphate Nutrition 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a method for preparing a high water dispersibility titanium dioxide. The method comprises the following steps sequentially: a, adding a dispersing agent into a titanium dioxide slurry, and stirring uniformly; b, adding a phosphorus-containing solution, and curing; c, adding an aluminum sulfate solution to control the pH value of the titanium dioxide slurry to be 1.5 to 4.5, and curing; d, adding a sodium metaaluminate solution to control the pH value of the titanium dioxide slurry to be 8.5 to 10.5, and curing; e, adjusting the pH value of the titanium dioxide slurry to be 7.0 to 7.8, and curing; f, filtering, washing, drying, and pulverizing to obtain the high water dispersibility titanium dioxide. According to the method, before coating, the dispersing agent is added to improve a dispersing condition of the titanium dioxide slurry, then the phosphorus-containing solution and the aluminum-containing solution are used as a coating agent, and then the coating agent is deposited on the surface of titanium dioxide in forms of aluminum phosphate and hydrated alumina, so that the water dispersibility of a product is effectively improved, and the titanium dioxide product with the high water dispersibility is obtained.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for preparing high-water-dispersibility titanium dioxide through surface treatment.
Background
Titanium dioxide is widely applied to the fields of paint, plastics, printing ink and paper making as a white pigment. The titanium dioxide is divided into a water-based system and an oil-based system according to the hydrophile-lipophile of the titanium dioxide system, in the application of the water-based titanium dioxide, the water dispersibility plays a key role in the application performance, particularly in the fields of water-based paint and paper making, if the water dispersibility of the titanium dioxide is good, the titanium dioxide has high covering power and good whiteness, and is beneficial to keeping the stability of the paint system for a long time, being convenient for transportation and storage and increasing the mechanical property of a coating film; if the water dispersibility of the titanium dioxide is poor, the titanium dioxide is easy to agglomerate after being dispersed in the coating to generate coarse phenomenon and delamination.
The prior art methods for improving the water dispersibility of titanium dioxide are usually organic coating or inorganic-organic coating treatment, such as coating silicon, aluminum or organic treatment of titanium dioxide products by adding hydrophilic treating agents such as TMP, but the steps are relatively complicated and the effect is not good.
According to the related literature and patent reports at present, no method for obtaining rutile type titanium dioxide with high water dispersibility by adopting a method of coating aluminum phosphate and aluminum oxide on an inorganic surface is available.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present invention to address one or more of the above mentioned technical problems.
The invention aims to provide a method for increasing the surface hydrophilicity of titanium dioxide and improving the water dispersibility of the titanium dioxide by coating aluminum phosphate and hydrated alumina on the surface of a primary rutile titanium dioxide product.
In order to achieve the above object, the present invention provides a method for preparing high water-dispersibility titanium dioxide, comprising the following steps performed in sequence: a. adding a dispersing agent into the titanium dioxide slurry, and uniformly stirring; b. adding a phosphorus-containing solution, and curing; c. adding an aluminum sulfate solution to control the pH value of the titanium dioxide slurry to be 1.5-4.5, and curing; d. adding a sodium metaaluminate solution to control the pH value of the titanium dioxide slurry to be 8.5-10.5, and curing; e. adjusting the pH value of the titanium dioxide slurry to 7.0-7.8, and curing; f. filtering, washing, drying and crushing to obtain the high-water-dispersibility titanium dioxide.
According to an embodiment of the method for preparing the high-water-dispersibility titanium dioxide, in the step a, the titanium dioxide slurry is obtained by pulping a rutile type titanium dioxide primary product with desalted water, and the concentration of the titanium dioxide slurry is 220-380 g/l.
According to an embodiment of the method for preparing the high-water-dispersibility titanium dioxide, in the step a, the temperature of the titanium dioxide slurry is 50-90 ℃.
According to one embodiment of the method for preparing high-water-dispersibility titanium dioxide, the dispersing agent is one or more of sodium silicate, sodium hexametaphosphate, monoethanol ammonium and ammonium dihydrogen phosphate.
According to one embodiment of the method for preparing high-water-dispersibility titanium dioxide, the dispersing agent is added in the amount of TiO in the titanium dioxide slurry20.05-0.25% of the mass.
According to one embodiment of the method for preparing high water dispersibility titanium dioxide, in the step b, the phosphorus-containing solution is one or more of phosphoric acid solution, sodium hexametaphosphate solution, trisodium phosphate solution and sodium pyrophosphate solution.
According to one embodiment of the method for preparing high-water-dispersibility titanium dioxide powder, in the step b, the adding amount of the phosphorus-containing solution is P2O5Is calculated and in accordance with P2O5With the TiO in the titanium dioxide slurry2The mass ratio of (A) to (B) is 2: 100-4: 100.
According to an embodiment of the method for preparing titanium dioxide with high water dispersibility, in step c, the aluminum sulfate solution is added in an amount of Al2O3Calculated and in accordance with Al2O3Is TiO in the titanium dioxide slurry21.0-3.2% of the mass; in step d, the addition amount of the sodium metaaluminate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry21.3-3.5% of the mass.
According to an embodiment of the method for preparing the high-water-dispersibility titanium dioxide, in the step e, dilute acid with the mass concentration of 10-20% is used for adjusting the pH value of the titanium dioxide slurry.
According to an embodiment of the method for preparing the high-water-dispersibility titanium dioxide, the curing time from the step b to the step e is 5-60 min, 10-110 min and 60-180 min in sequence.
Compared with the prior art, the invention has the beneficial effects that: the dispersing state of the titanium dioxide slurry is improved by adding a dispersing agent before coating, then a phosphorus-containing solution and an aluminum-containing solution are used as coating agents, and then the coating agents are deposited on the surface of titanium dioxide in the form of aluminum phosphate and hydrated alumina, so that the water dispersibility of the titanium dioxide slurry is effectively improved, and the titanium dioxide product with high water dispersibility is obtained.
Detailed Description
Hereinafter, the method for preparing high water dispersibility titanium dioxide according to the present invention will be described in detail.
The method for preparing the titanium dioxide with high water dispersibility is mainly used for carrying out surface treatment on rutile titanium dioxide to improve the water dispersibility of the rutile titanium dioxide. The content described herein is mass percentage content, and the means for characterizing the water dispersibility of titanium dioxide in the present invention specifically refers to the water dispersibility detection method in the example, but the present invention is not limited thereto, as long as the method can quantitatively determine the water dispersibility of titanium dioxide.
The method for preparing the high-water-dispersibility titanium dioxide powder according to the exemplary embodiment of the invention comprises the following steps a-f which are sequentially executed:
a. and adding a dispersing agent into the titanium dioxide slurry, and uniformly stirring.
Wherein, the titanium dioxide slurry is obtained by pulping the primary rutile titanium dioxide with desalted water. According to one embodiment of the invention, the concentration of the titanium dioxide slurry is 220-380 g/l, preferably 280-300 g/l. In order to improve the blending effect, the temperature of the titanium dioxide slurry can be controlled to be 50-90 ℃, and preferably controlled to be 60-70 ℃. The temperature of the titanium dioxide slurry is controlled to control the speed of the acid and alkali neutralization reaction of the coating agent so as to control the deposition rate of the coating layer.
The dispersing agent can be added to improve the dispersion condition of the titanium dioxide slurry, and can be one or more of sodium silicate, sodium hexametaphosphate, mono-ethanol ammonium and ammonium dihydrogen phosphate. According to one embodiment of the invention, the dispersant is added in an amount of TiO in the titanium dioxide slurry20.05 to 0.25% by mass, preferably 0.10 to 0.15% by mass. The dispersant is added to achieve the best dispersion effect, and if the amount of the dispersant is small, the dispersion effect is not good, and if the amount of the dispersant is high, the cost is high. Generally, the dispersant is generally added in the form of a solution, for example, with a mass concentration of 10 to 25%.
b. Adding phosphorus-containing solution, and aging.
And adding a phosphorus-containing solution into the titanium dioxide slurry added with the dispersing agent, wherein the phosphorus-containing solution is added as a coating agent. According to the invention, the phosphorus-containing solution can be one or more of a phosphoric acid solution, a sodium hexametaphosphate solution, a trisodium phosphate solution and a sodium pyrophosphate solution, and the adding amount of the phosphorus-containing solution is P2O5Calculate and follow P2O5With TiO in titanium dioxide slurry2The mass ratio of (A) to (B) is 2: 100-4: 100. Wherein, the common practice in the titanium white industry is to calculate the phosphorus-containing solution as phosphorus pentoxideThe calculation method is well known to those skilled in the art.
After the phosphorus-containing solution is added, curing is carried out for 5-60 min, preferably for 20-30 min. The curing process in the step does not have chemical reaction, and is only used for uniformly dispersing the coating agent in the system.
c. Adding an aluminum sulfate solution to control the pH value of the titanium dioxide slurry to be 1.5-4.5, and curing.
And adding an aluminum sulfate solution into the titanium dioxide slurry, wherein the aluminum sulfate solution is also added as a coating agent, and the aluminum sulfate reacts with phosphate ions in the phosphorus-containing solution added before to obtain aluminum phosphate precipitate. According to the invention, the aluminium sulphate solution is added in an amount of Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry21.0-3.2% of the mass.
The pH value of the titanium dioxide slurry is controlled to be 1.5-4.5, so that aluminum phosphate obtained by reacting the phosphorus-containing solution with the aluminum sulfate solution is better deposited on the surface of the titanium dioxide, and if the pH value is too low, the deposited aluminum phosphate is dissolved.
After adding aluminum sulfate solution, curing for 10-110 min, preferably 50-60 min. The aging process in the step is to allow the phosphorus-containing solution and the aluminum sulfate solution to fully react to obtain the aluminum phosphate and fully deposit the aluminum phosphate.
d. Adding sodium metaaluminate solution to control the pH value of the titanium dioxide slurry to be 8.5-10.5, and curing.
And then, adding a sodium metaaluminate solution into the titanium dioxide slurry, wherein the sodium metaaluminate solution is also added as a coating agent, the sodium metaaluminate can react with water, sulfate ions and the like to obtain hydrated alumina, namely an aluminum hydroxide precipitate, and in addition, the sodium metaaluminate can also react with phosphate ions to obtain a small part of aluminum phosphate precipitate. According to the invention, the sodium metaaluminate solution is added in an amount of Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry21.3-3.5% of the mass. Wherein,the calculation of sodium metaaluminate as alumina is a common practice in the titanium white industry and is well known to those skilled in the art.
The pH value of the titanium dioxide slurry is controlled to be 8.5-10.5, so that the generated hydrated alumina is continuously deposited on the surface of the titanium dioxide in a boehmite type under an alkaline condition, and the dispersibility of the titanium dioxide slurry is improved. If the pH value is too low, the viscosity of the coating system is high, the deposition uniformity of the coating agent on the surface of titanium dioxide is not facilitated, and if the pH value is too high, the aluminum phosphate deposited in the previous step is dissolved by alkali.
And (3) adding a sodium metaaluminate solution, and then curing for 10-110 min, preferably 50-60 min. The aging in the step is to allow the sodium metaaluminate to fully react to obtain hydrated alumina and fully deposit the hydrated alumina.
e. Adjusting the pH value of the titanium dioxide slurry to 7.0-7.8, and curing.
And finally, adjusting the pH value of the titanium dioxide slurry to 7.0-7.8 to adjust the pH value of the titanium dioxide slurry to be neutral. Because under the neutral condition, the titanium dioxide slurry is easy to wash, and the titanium dioxide is required to be neutral when in application. According to the invention, dilute acid with the mass concentration of 10-20% such as sulfuric acid or hydrochloric acid can be adopted to adjust the pH value of the titanium dioxide slurry.
After the pH value is adjusted, curing is carried out for 60-180 min, preferably 110-120 min. The aging in the step is to further deposit hydrated alumina and improve the deposition rate of aluminum.
f. Filtering, washing, drying and crushing to obtain the high-water-dispersibility titanium dioxide.
In order that the above-described exemplary embodiments of the invention may be better understood, further description thereof with reference to specific examples is provided below.
First, the method for detecting water dispersibility employed in the present invention will be described in detail:
two weighing bottles are taken and dried in an oven to constant weight, and the weighing bottles are respectively marked as 1#And 2#Weighing constant weight 1#And 2#Bottle, mass respectively marked m1And m2。
Weighing 15.00g of sample to be tested in a 500ml conical flask, adding 285.00g of distilled water, plugging a rubber stopper, placing on a speed-regulating multi-purpose oscillator for oscillation and dispersion for 30 minutes, measuring 10ml of dispersed sample slurry to be tested by using a 10ml pipette, placing the sample slurry to 1#In the weighing bottle, accurately weigh on an electronic balance, and the mass is recorded as m3。
200ml of the dispersed slurry was measured out using a 250ml measuring cylinder, and allowed to stand and settle naturally for 5 hours.
After the sedimentation is finished, using a 50ml pipette to transfer 175ml of supernatant liquid from a 250ml measuring cylinder (the supernatant liquid is transferred from top to bottom gradually when the supernatant liquid is transferred, and the slurry at the bottom of the measuring cylinder can not be taken), placing the obtained supernatant liquid in a 500ml conical flask, oscillating and dispersing for 30 minutes on a speed-regulating multipurpose oscillator, using a 10ml pipette to measure 10ml of dispersed titanium dioxide slurry, placing the obtained product in a 2 ml conical flask#In the weighing bottle, accurately weighing on a one-ten-thousandth balance, and recording the mass as m4。
Will 1#And 2#The bottle was placed in an oven with the slurry and dried at 145 + -5 deg.C for 2.5 hours.
Drying the obtained product 1#And 2#The sample was placed in a desiccator for 30 minutes and then taken out, and weighed on an electronic balance, 1#Is marked as m5，2#Is marked as m6。
The water dispersibility is calculated by the formula:
example 1:
taking 1000g of primary rutile titanium dioxide which is not subjected to post-treatment, pulping by using desalted water, wherein the concentration of titanium dioxide slurry obtained after pulping is 280g/l,heating the titanium dioxide slurry to 50 ℃; then adding a sodium silicate solution with the mass concentration of 18% into the heated titanium dioxide slurry, and uniformly stirring, wherein the adding amount of the sodium silicate solution is TiO in the titanium dioxide slurry20.08% by mass; adding sodium hexametaphosphate solution, wherein the adding amount of the sodium hexametaphosphate solution is P2O5Calculated and in mass ratio of P2O5：TiO2Calculating the ratio of 2.5:100, and curing for 15 min; adding aluminum sulfate solution, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry2Calculating the mass of 2.5%, controlling the pH value of the titanium dioxide slurry to be 1.65, and curing for 60 min; then adding sodium metaaluminate solution, wherein the adding amount of the sodium metaaluminate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry2Calculating the mass of 3.0 percent, controlling the pH value of the titanium dioxide slurry to be 10.05, and curing for 60 min; adjusting the pH value of the titanium dioxide slurry to 7.25 by using dilute sulfuric acid with the mass concentration of 15%, and curing for 120 min; and finally, filtering, washing, drying and crushing the solution to obtain a titanium dioxide product. Through detection, the water dispersibility of the obtained titanium dioxide is 97.80%.
Example 2:
taking 1000g of a primary rutile titanium dioxide product which is not subjected to post-treatment, pulping by using desalted water, wherein the concentration of titanium dioxide slurry obtained after pulping is 300g/l, and heating the titanium dioxide slurry to 60 ℃; then adding ammonium dihydrogen phosphate solution with mass concentration of 18% into the heated titanium dioxide slurry, and uniformly stirring, wherein the adding amount of the ammonium dihydrogen phosphate is TiO in the titanium dioxide slurry20.25% of the mass; adding phosphoric acid solution, wherein the adding amount of the phosphoric acid solution is P2O5Calculated and in mass ratio of P2O5：TiO2Aging for 60min, calculated as 2.0: 100; adding aluminum sulfate solution, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry21.0% calculation of the massControlling the pH value of the titanium dioxide slurry to be 3.7, and curing for 10 min; then adding sodium metaaluminate solution, wherein the adding amount of the sodium metaaluminate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry2When the mass is 3.5%, controlling the pH value of the titanium dioxide slurry to be 10.38, and curing for 30 min; adjusting the pH value of the titanium dioxide slurry to 7.45 by using 20% dilute hydrochloric acid, and curing for 60 min; and finally, filtering, washing, drying and crushing the solution to obtain a titanium dioxide product. Through detection, the water dispersibility of the obtained titanium dioxide is 96.70%.
Example 3:
taking 1000g of a primary rutile titanium dioxide product which is not subjected to post-treatment, pulping by using desalted water, wherein the concentration of titanium dioxide slurry obtained after pulping is 380g/l, and heating the titanium dioxide slurry to 80 ℃; then adding a sodium hexametaphosphate solution with the mass concentration of 20 percent into the heated titanium dioxide slurry, and uniformly stirring, wherein the addition amount of the sodium hexametaphosphate is TiO in the titanium dioxide slurry20.15% of the mass; adding trisodium phosphate solution, wherein the addition amount of the trisodium phosphate solution is P2O5Calculated and in mass ratio of P2O5：TiO2Aging for 30min, calculated as 4.0: 100; adding aluminum sulfate solution, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry2Calculating the mass of 3.2%, controlling the pH value of the titanium dioxide slurry to be 2.3, and curing for 60 min; then adding sodium metaaluminate solution, wherein the adding amount of the sodium metaaluminate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry2Calculating the mass of 1.5%, controlling the pH value of the titanium dioxide slurry to be 8.8, and curing for 110 min; adjusting the pH value of the titanium dioxide slurry to 7.56 by using dilute sulfuric acid with the mass concentration of 20%, and curing for 180 min; and finally, filtering, washing, drying and crushing the solution to obtain a titanium dioxide product. Through detection, the water dispersibility of the obtained titanium dioxide is 98.20%.
Example 4:
taking 1000g of a primary rutile titanium dioxide product which is not subjected to post-treatment, pulping by using desalted water, wherein the concentration of titanium dioxide slurry obtained after pulping is 220g/l, and heating the titanium dioxide slurry to 90 ℃; then adding a monoethanolamine solution with the mass concentration of 25% into the heated titanium dioxide slurry, and uniformly stirring, wherein the addition amount of the dispersant monoethanolamine sodium is TiO in the titanium dioxide slurry20.20% of the mass; adding sodium pyrophosphate solution, adding trisodium phosphate solution in an amount of P2O5Calculated and in mass ratio of P2O5：TiO2Aging for 30min, calculated as 3.2: 100; adding aluminum sulfate solution, wherein the adding amount of the aluminum sulfate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry2Calculating the mass of 2.6%, controlling the pH value of the titanium dioxide slurry to be 3, and curing for 110 min; then adding sodium metaaluminate solution, wherein the adding amount of the sodium metaaluminate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry2Calculating the mass of 2.2%, controlling the pH value of the titanium dioxide slurry to be 9.56, and curing for 10 min; adjusting the pH value of the titanium dioxide slurry to 7.8 by using 20% dilute hydrochloric acid, and curing for 120 min; and finally, filtering, washing, drying and crushing the solution to obtain a titanium dioxide product. Through detection, the water dispersibility of the obtained titanium dioxide is 96.30%.
In conclusion, the dispersing agent is added before coating to improve the dispersion condition of the titanium dioxide slurry, and then the phosphorus-containing solution and the aluminum-containing solution are used as the coating agent, and the coating agent is deposited on the surface of titanium dioxide in the form of aluminum phosphate and hydrated alumina, so that the water dispersibility of the product is improved.
Although the present invention has been described above in connection with exemplary embodiments, it will be apparent to those skilled in the art that various modifications and changes may be made to the exemplary embodiments of the present invention without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The method for preparing the high-water-dispersibility titanium dioxide is characterized by comprising the following steps in sequence:
a. adding a dispersing agent into the titanium dioxide slurry, and uniformly stirring;
b. adding a phosphorus-containing solution, and curing;
c. adding an aluminum sulfate solution to control the pH value of the titanium dioxide slurry to be 1.5-4.5, and curing;
d. adding a sodium metaaluminate solution to control the pH value of the titanium dioxide slurry to be 8.5-10.5, and curing;
e. adjusting the pH value of the titanium dioxide slurry to 7.0-7.8, and curing;
f. filtering, washing, drying and crushing to obtain the high-water-dispersibility titanium dioxide.
2. The method for preparing high-water-dispersibility titanium dioxide according to claim 1, wherein in the step a, the titanium dioxide slurry is obtained by pulping a rutile type titanium dioxide primary product with desalted water, and the concentration of the titanium dioxide slurry is 220-380 g/l.
3. The method for preparing high-water-dispersibility titanium dioxide according to claim 1, wherein in the step a, the temperature of the titanium dioxide slurry is 50-90 ℃.
4. The method for preparing high-water-dispersibility titanium dioxide according to claim 1, wherein the dispersant is one or more of sodium silicate, sodium hexametaphosphate, mono ethanol ammonium and ammonium dihydrogen phosphate.
5. The method for preparing high-water-dispersibility titanium dioxide according to claim 1 or 4, wherein the dispersant is added in an amount of TiO in the titanium dioxide slurry20.05-0.25% of the mass.
6. The method for preparing high-water-dispersibility titanium dioxide according to claim 1, wherein in the step b, the phosphorus-containing solution is one or more of phosphoric acid solution, sodium hexametaphosphate solution, trisodium phosphate solution and sodium pyrophosphate solution.
7. The method for preparing high water dispersibility titanium dioxide according to claim 1 or 6, wherein in step b, the phosphorus-containing solution is added in an amount P2O5Is calculated and in accordance with P2O5And T in the titanium dioxide slurryiO2The mass ratio of (A) to (B) is 2: 100-4: 100.
8. The method for preparing high-water-dispersibility titanium dioxide according to claim 1, wherein in step c, the aluminum sulfate solution is added in an amount of Al2O3Calculated and in accordance with Al2O3Is TiO in the titanium dioxide slurry21.0-3.2% of the mass; in step d, the addition amount of the sodium metaaluminate solution is Al2O3Calculated and in accordance with Al2O3Is TiO in titanium dioxide slurry21.3-3.5% of the mass.
9. The method for preparing high-water-dispersibility titanium dioxide according to claim 1, wherein in the step e, dilute acid with the mass concentration of 10-20% is used for adjusting the pH value of the titanium dioxide slurry.
10. The method for preparing high-water-dispersibility titanium dioxide according to claim 1, wherein the curing time from step b to step e is 5-60 min, 10-110 min and 60-180 min in sequence.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410165452.5A CN103965659B (en) | 2014-04-23 | 2014-04-23 | A kind of method preparing high-dispersed titanium pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410165452.5A CN103965659B (en) | 2014-04-23 | 2014-04-23 | A kind of method preparing high-dispersed titanium pigment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103965659A true CN103965659A (en) | 2014-08-06 |
| CN103965659B CN103965659B (en) | 2015-11-04 |
Family
ID=51235681
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410165452.5A Active CN103965659B (en) | 2014-04-23 | 2014-04-23 | A kind of method preparing high-dispersed titanium pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103965659B (en) |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194409A (en) * | 2014-08-13 | 2014-12-10 | 攀钢集团钛业有限责任公司 | High-temperature-resistant titanium white, and preparation method and application thereof |
| CN104194412A (en) * | 2014-09-23 | 2014-12-10 | 安徽金星钛白（集团）有限公司 | High coulombic efficiency TiO2 preparation method |
| CN104194410A (en) * | 2014-08-15 | 2014-12-10 | 攀钢集团钛业有限责任公司 | Preparation method of titanium dioxide pigment |
| CN104877393A (en) * | 2015-04-08 | 2015-09-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium dioxide with low oil absorption and preparation method of titanium dioxide |
| CN105504885A (en) * | 2014-09-26 | 2016-04-20 | 河南佰利联化学股份有限公司 | Preparation method for special rutile titanium dioxide used for papermaking |
| CN106947294A (en) * | 2017-03-14 | 2017-07-14 | 襄阳龙蟒钛业有限公司 | A kind of production method of high fluidity titanium dioxide |
| CN107163623A (en) * | 2017-06-27 | 2017-09-15 | 安徽金星钛白（集团）有限公司 | It is a kind of to have high thermal stability and the titanium white powder, preparation method thereof of covering power concurrently |
| CN108587244A (en) * | 2018-04-25 | 2018-09-28 | 四川龙蟒钛业股份有限公司 | A kind of titanium dioxide aluminium coating process with cost advantage |
| CN108997789A (en) * | 2018-09-05 | 2018-12-14 | 攀枝花大互通钛业有限公司 | A kind of compound modified titanium and preparation method thereof |
| CN108997788A (en) * | 2018-08-27 | 2018-12-14 | 攀钢集团重庆钛业有限公司 | The preparation method of high covering power titanium dioxide |
| CN109535775A (en) * | 2018-12-24 | 2019-03-29 | 攀钢集团重庆钛业有限公司 | The preparation method of ink tailored version titanium dioxide |
| CN113789067A (en) * | 2021-10-22 | 2021-12-14 | 攀钢集团重庆钒钛科技有限公司 | Preparation method of high-water-dispersibility titanium dioxide slurry |
| CN113999545A (en) * | 2021-12-02 | 2022-02-01 | 攀钢集团重庆钛业有限公司 | Titanium dioxide for high-light-resistance decorative paper and preparation method thereof |
| CN114264577A (en) * | 2021-12-30 | 2022-04-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for rapidly detecting dispersion stability of nano titanium dioxide in oil phase |
| CN115537043A (en) * | 2022-09-22 | 2022-12-30 | 广西金茂钛业有限公司 | Method for preparing titanium dioxide for papermaking |
| CN115651426A (en) * | 2022-10-24 | 2023-01-31 | 攀钢集团研究院有限公司 | Method for preparing titanium white special for printing ink by using hydrochloric acid as chlorination byproduct |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006012564B4 (en) * | 2006-03-16 | 2008-11-06 | Kronos International, Inc. | Titanium dioxide pigment coated with hollow microspheres and method of manufacture |
| CN101857736B (en) * | 2010-07-16 | 2012-10-10 | 四川龙蟒钛业股份有限公司 | Production method of high-light-fastness rutile type titanium dioxide |
| CN102532952B (en) * | 2011-12-30 | 2013-11-27 | 锦州钛业有限公司 | Preparation method of titanium dioxide pigment special for laminated paper |
| CN103113762B (en) * | 2013-02-25 | 2014-11-26 | 南京钛白化工有限责任公司 | Method for preparing high-light-resistance decorative laminated paper titanium pigment |
| CN103709792B (en) * | 2013-12-06 | 2015-07-15 | 攀钢集团钛业有限责任公司 | Preparation method for titanium dioxide pigment |
-
2014
- 2014-04-23 CN CN201410165452.5A patent/CN103965659B/en active Active
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194409A (en) * | 2014-08-13 | 2014-12-10 | 攀钢集团钛业有限责任公司 | High-temperature-resistant titanium white, and preparation method and application thereof |
| CN104194410A (en) * | 2014-08-15 | 2014-12-10 | 攀钢集团钛业有限责任公司 | Preparation method of titanium dioxide pigment |
| CN104194412A (en) * | 2014-09-23 | 2014-12-10 | 安徽金星钛白（集团）有限公司 | High coulombic efficiency TiO2 preparation method |
| CN105504885A (en) * | 2014-09-26 | 2016-04-20 | 河南佰利联化学股份有限公司 | Preparation method for special rutile titanium dioxide used for papermaking |
| CN104877393A (en) * | 2015-04-08 | 2015-09-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium dioxide with low oil absorption and preparation method of titanium dioxide |
| CN106947294A (en) * | 2017-03-14 | 2017-07-14 | 襄阳龙蟒钛业有限公司 | A kind of production method of high fluidity titanium dioxide |
| CN107163623A (en) * | 2017-06-27 | 2017-09-15 | 安徽金星钛白（集团）有限公司 | It is a kind of to have high thermal stability and the titanium white powder, preparation method thereof of covering power concurrently |
| CN108587244B (en) * | 2018-04-25 | 2020-03-20 | 四川龙蟒钛业股份有限公司 | Titanium dioxide aluminum coating process with cost advantage |
| CN108587244A (en) * | 2018-04-25 | 2018-09-28 | 四川龙蟒钛业股份有限公司 | A kind of titanium dioxide aluminium coating process with cost advantage |
| CN108997788A (en) * | 2018-08-27 | 2018-12-14 | 攀钢集团重庆钛业有限公司 | The preparation method of high covering power titanium dioxide |
| CN108997789A (en) * | 2018-09-05 | 2018-12-14 | 攀枝花大互通钛业有限公司 | A kind of compound modified titanium and preparation method thereof |
| CN109535775A (en) * | 2018-12-24 | 2019-03-29 | 攀钢集团重庆钛业有限公司 | The preparation method of ink tailored version titanium dioxide |
| CN109535775B (en) * | 2018-12-24 | 2020-11-24 | 攀钢集团重庆钛业有限公司 | Preparation method of titanium dioxide special for printing ink |
| CN113789067A (en) * | 2021-10-22 | 2021-12-14 | 攀钢集团重庆钒钛科技有限公司 | Preparation method of high-water-dispersibility titanium dioxide slurry |
| CN113999545A (en) * | 2021-12-02 | 2022-02-01 | 攀钢集团重庆钛业有限公司 | Titanium dioxide for high-light-resistance decorative paper and preparation method thereof |
| CN114264577A (en) * | 2021-12-30 | 2022-04-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for rapidly detecting dispersion stability of nano titanium dioxide in oil phase |
| CN115537043A (en) * | 2022-09-22 | 2022-12-30 | 广西金茂钛业有限公司 | Method for preparing titanium dioxide for papermaking |
| CN115651426A (en) * | 2022-10-24 | 2023-01-31 | 攀钢集团研究院有限公司 | Method for preparing titanium white special for printing ink by using hydrochloric acid as chlorination byproduct |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103965659B (en) | 2015-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103965659A (en) | Method for preparing high water dispersibility titanium dioxide | |
| CN103555001B (en) | Method for coating titanium dioxide | |
| CN104194410A (en) | Preparation method of titanium dioxide pigment | |
| FI89191B (en) | BULKPIGMENTUPPSLAMNING OCH FOERFARANDE FOER FRAMSTAELLNING AV DEN | |
| JP5237830B2 (en) | Titanium dioxide pigment having high opacity and method for producing the same | |
| CN103709792B (en) | Preparation method for titanium dioxide pigment | |
| CN105062150A (en) | Treatment method capable of improving weather resistance of titanium dioxide | |
| US20080076838A1 (en) | Methods of preparing silica sols, and stable high-solids silica sols prepared thereby | |
| CN102070921A (en) | Method for preparing special titanium dioxide pigment for plastic sectional materials by chlorination method | |
| BR112013025092B1 (en) | PROCESS FOR THE PRODUCTION OF A POST-TREATED TITANIUM DIOXIDE PIGMENT | |
| BRPI0509204B1 (en) | process to produce an aqueous silica-based sun. | |
| CN108997788A (en) | The preparation method of high covering power titanium dioxide | |
| CN107353673A (en) | Titanium dioxide that surface is modified and preparation method thereof | |
| CN102099291A (en) | Silica-based sols | |
| CN108997789A (en) | A kind of compound modified titanium and preparation method thereof | |
| Zhang et al. | Influence of some additives to aluminium species distribution in aluminium coagulants | |
| CN105504885A (en) | Preparation method for special rutile titanium dioxide used for papermaking | |
| BR112016009559B1 (en) | PROCESS FOR THE PRODUCTION OF COMPOSITE PARTICLES AND USE THEREOF | |
| BR112014029985B1 (en) | TITANIUM DIOXIDE PIGMENT PARTICLES, PROCESS FOR THE SURFACE TREATMENT OF THEM AND THEIR USE | |
| TWI639659B (en) | Method for coating the surface of inorganic particles, particularly titanium dioxide pigment particles | |
| CN104387809A (en) | Inorganic enveloping method for rutile titanium dioxide | |
| KR102710313B1 (en) | Phenylphosphonic acid-containing silica sol and its use | |
| CN102502932B (en) | High-effective composite flocculant for treating low-turbidity water and preparation method of high-effective composite flocculant | |
| CN101298346B (en) | Polysilicate aluminum sulphate flocculant, preparation process and use thereof | |
| CN104402058B (en) | A kind of poly-aluminum ferric chloride sulfate filtering residue recycling technique |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |